高等学校化学学报 ›› 2000, Vol. 21 ›› Issue (2): 286.

• 研究快报 • 上一篇    下一篇

吡啶-2-羧酸钴催化氯苄双羰化合成新型α-酮酸研究

李光兴, 黄汉民   

  1. 华中理工大学化学系, 武汉 430074
  • 收稿日期:1999-09-15 出版日期:2000-02-24 发布日期:2000-02-24
  • 通讯作者: 李光兴(1951年出生),男,副教授,主要从事均相催化及C1化学研究.E-mail:guangx in@wuhan.cngb.com E-mail:guangx in@wuhan.cngb.com
  • 基金资助:

    湖北省重点科技攻关项目(批准号:991P0315)资助

Double Carbonylation of Benzyl Chloride to Substituted Phenylpyruvic Acid Catalyzed by Cobalt Pyridine-2-carboxylate

LI Guang-Xing, HUANG Han-Min   

  1. Department of Chemistry, Huazhong University of Science and Technology, Wuhan 430074, China
  • Received:1999-09-15 Online:2000-02-24 Published:2000-02-24

关键词: 吡啶-2-羧酸钴, &alpha, -酮酸, 双羰化

Abstract: The complex cobalt pyridine-2-carboxylate Co(Pyca)2·4H2Ocatalyst is found to have a good activity and selectivity for double carbonylation of benzyl chloride to a substituted phenylpyruvic acid, β-benzyl-αphenylpyruvic acid, in CaO/CH3OH/H2Oreaction system. After stirring 10h in3.0 MPa and 333 Kwith the PhCH2Cl to CaOratio of 1.33 and catalyst of 5.5 mmol, the yield of the substituted phenylpyruvic acid is 40%, the selectivity is 80%, and the conversion of benzyl chloride is 51%. The substituted phenylpyruvic acid is characterized by IR, NMR, MSand microanalyses. The strong IRbands at 3453-3554 cm-1are assigned to the -COOH , and the sharp bands at 1706 and 1729 cm-1are assigned to the two C=Ogroups stretch, respectively. In the 13C NMRspectra, two characteristic strong peaks at δ 193.2 and 159.2 are assigned to C=Oand COOH. The MSspectra shows that the main characteristic peaks are m/z=254(M+), 236, 209, 181(basic peak), 91 and 77. The melting point of the phenylpyruvic acid is 87-89 ℃. Further study of the double carbonylation reaction over this new catalyst system is being carried out.

Key words: Cobalt bis(2-pyridinecarboxylate)-tetrahydrate, Substituted phenylpyruvic acid, Double carbonylation

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